Methanol → HCID 19095906, 화합물

HRID 486774노트

반응식

HRID 486774 반응식
C[Si](C)(C)[NH:3][Si](C)(C)C.CO.[C:12]([O:16][C:17]([N:19]1[CH2:51][CH2:50][C:21]2([CH2:49][N:24]3[C:25]4[CH:26]=[CH:27][CH:28]=[CH:29][C:30]=4[C:31]([C:32]4[C:33](=O)[O:34][C:35](=[O:47])[C:36]=4[C:37]4[C:45]5[C:40](=[CH:41][CH:42]=[CH:43][CH:44]=5)[N:39]([CH3:46])[CH:38]=4)=[C:23]3[CH2:22]2)[CH2:20]1)=[O:18])([CH3:15])([CH3:14])[CH3:13]>CN(C=O)C>[C:12]([O:16][C:17]([N:19]1[CH2:51][CH2:50][C:21]2([CH2:49][N:24]3[C:25]4[CH:26]=[CH:27][CH:28]=[CH:29][C:30]=4[C:31]([C:32]4[C:33](=[O:34])[NH:3][C:35](=[O:47])[C:36]=4[C:37]4[C:45]5[C:40](=[CH:41][CH:42]=[CH:43][CH:44]=5)[N:39]([CH3:46])[CH:38]=4)=[C:23]3[CH2:22]2)[CH2:20]1)=[O:18])([CH3:14])([CH3:13])[CH3:15]

참가 물질

5

반응물 3

HCID 887MethanolHCID 13838HexamethyldisilazaneHCID 19095911HCID 19095911, 화합물

생성물 1

HCID 19095906HCID 19095906, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 0.59 ml of 1,1,1,3,3,3-hexamethyldisilazane and 45 mg of methanol was added to a solution of 150 mg of 3-[1-(tert.butoxy-carbonyl)-1',3'-dihydrospiro[pyrrolidine-3,2'-pyrrolo[1,2-a]indol]-9'-yl]-4-(1-methyl-3-indolyl)-furan-2,5-dione in 10 ml of DMF and stirred for 72 hours. The solvent was removed by evaporation and the residue was treated with 10 ml of methanol. After evaporation, the residue was subjected to chromatography on silica gel using dichloromethane/ethyl acetate (4:1) for the elution. There were obtained 120 mg of 3-[1-(tert.butoxycarbonyl)-1',3'-dihydrospiro[pyrrolidine-3,2'-pyrrolo[1,2-a]indol]-9'-yl]-4-(1-methyl-3-indolyl)-1H-pyrrole-2,5-dione of melting point 232°-235° C.

후처리

  1. customThe solvent was removed by evaporation
  2. additionthe residue was treated with 10 ml of methanol
  3. customAfter evaporation
  4. washfor the elution

출처 및 근거

ORD 기록
ord-40352807988843ab824a05561f4f43a2
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05292747

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